Three-dimensional porous copper sulfide aerogel as well as preparation method and application thereof
A three-dimensional porous copper sulfide technology, applied in chemical instruments and methods, preparation of test samples, colloid chemistry, etc., can solve the problems of low yield of nanostructured materials, insufficient specific surface area, and fine powder particles, etc., to achieve Improve separation convenience, high specific surface area, and good selectivity
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Embodiment 1
[0067] Preparation of three-dimensional porous copper sulfide aerogel materials:
[0068] (1) Take 3-5nm copper sulfide nanocrystals as the initial structural unit. First, 1 to 3 mmol of CuCl 2 ·2H 2 O was dissolved in 10-20 mL of oleylamine (80-90%) and toluene (AR) solution and sonicated until dissolved. Add 300 to 600 μL of (NH 4 ) 2 S aqueous solution (20%) was added to the above solution, and with magnetic stirring, 20 mL of absolute ethanol was added after 1 min to stop the growth of nanocrystals. Centrifuge and disperse in n-hexane.
[0069] (2) 10 to 20 mg L of 5 to 15 mL -1 Na 2 The MFA solution of S is mixed with the above dispersion liquid, stirred at room temperature for 5-20 min, and then mixed with S 2- The ligands replace the oleylamine ligands around the copper sulfide nanocrystals, wash with n-hexane for 2 to 4 times, and the mixed solution of acetone and n-hexane will complete the ligand-exchanged S 2- The encapsulated copper sulfide nanocrystals wer...
Embodiment 2
[0075] Adsorption and enrichment of mercury ions in water by three-dimensional porous copper sulfide aerogel materials:
[0076] 3 mg of the three-dimensional porous copper sulfide aerogel material prepared in Example 1 (1) above was placed in a 50 mL small glass bottle, and 35 mL containing 13 mg L -1 A water sample of mercury ions was injected into the above-mentioned vial. After 15s, 30s, 60s, 120s and 300s of adsorption and enrichment, the three-dimensional porous copper sulfide aerogel material adsorbed with mercury ions was separated from the water body. The residual concentration of mercury ions in the water was analyzed and detected by ICP or ICP-MS method, and then the adsorption and enrichment rate of mercury ions was obtained. After calculation, the enrichment rates of three-dimensional porous copper sulfide aerogel materials at 15s, 30s, 60s, 120s and 300s are 97.3%, 98.8%, 98.9%, 100% and 100%, respectively. The relationship between the mercury ion enrichment ra...
Embodiment 3
[0078] The enrichment and separation of three-dimensional porous copper sulfide aerogel materials for different initial concentrations of mercury ions:
[0079] At room temperature (25°C), 2.5 mg of the three-dimensional porous copper sulfide aerogel material prepared in the above Example 1 was dispersed in a 20 mL water sample, and the initial concentration of mercury ions in the water sample was 10 mg L respectively. -1 , 50mg L -1 , 100mg L -1 , 200 mgL -1 , 300mg L -1 , 400mg L -1 . Adsorption and enrichment were carried out for 5 min to make the adsorption reach equilibrium. After adsorption is complete, the enriched material is separated from the water sample. The residual concentration of mercury ions in the water sample was detected by ICP or ICP-MS analysis, and then the adsorption and enrichment amount of mercury ions by the material was obtained. The result is as Figure 5 The maximum adsorption capacity of the three-dimensional porous copper sulfide aerogel...
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